Poly[[tetra­deca­kis­(μ-propionato)hepta­barium] propionic acid monosolvate tetra­hydrate]

The structure of the title compound is held together by Ba—O—Ba bonds as well as by O—H...O hydrogen bonds of moderate strength. There is an occupationally as well as a positionally disordered mol­ecule of propionic acid in the structure. Its occupation deviates from a potentially full occupation while the disordered mol­ecules occupy two positions related by a twofold rotation axis.

Key indicators

• Single-crystal X-ray study
• T = 95 K
• Mean [sigma](C-C) = 0.005 Å
• H-atom completeness 96%
• Disorder in main residue
• R factor = 0.028
• wR factor = 0.071
• Data-to-parameter ratio = 21.0

checkCIF/PLATON results

No syntax errors found



Alert level A
TYPE071_ALERT_1_A  _refine_ls_R_factor_gt is not of type numb.

Alert level B
PLAT213_ALERT_2_B Atom C18             has ADP max/min Ratio .....        4.3 prolat
PLAT315_ALERT_2_B Singly Bonded Carbon Detected (H-atoms Missing).       C24A Check

Alert level C
PLAT041_ALERT_1_C Calc. and Reported SumFormula    Strings  Differ     Please Check
PLAT043_ALERT_1_C Calculated and Reported Mol. Weight Differ by ..       3.78 Check
PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)...     Please Check
PLAT220_ALERT_2_C NonSolvent Resd 1  C   Ueq(max) / Ueq(min) Range        5.6 Ratio
PLAT220_ALERT_2_C NonSolvent Resd 1  O   Ueq(max) / Ueq(min) Range        5.6 Ratio
PLAT222_ALERT_3_C NonSolvent Resd 1  H   Uiso(max)/Uiso(min) Range        4.4 Ratio
PLAT260_ALERT_2_C Large Average Ueq of Residue Including      C24A      0.163 Check
PLAT309_ALERT_2_C Single Bonded Oxygen (C-O > 1.3 Ang) ...........        O16 Check
PLAT314_ALERT_2_C Small Angle for H2O: Metal-O1W      -H1O1W     .      80.48 Degree
PLAT411_ALERT_2_C Short Inter H...H Contact  H1C20    ..H2C23B   .       2.11 Ang.
                                          3/2-x,1/2-y,1/2+z  =      2_655 Check
PLAT906_ALERT_3_C Large K Value in the Analysis of Variance ......      2.468 Check
PLAT911_ALERT_3_C Missing FCF Refl Between Thmin & STh/L=    0.600         43 Report
PLAT971_ALERT_2_C Check Calcd Resid. Dens.  0.85A   From Ba2             1.73 eA-3
PLAT971_ALERT_2_C Check Calcd Resid. Dens.  0.81A   From Ba1             1.53 eA-3
PLAT975_ALERT_2_C Check Calcd Resid. Dens.  1.04A   From O5              0.72 eA-3
PLAT976_ALERT_2_C Check Calcd Resid. Dens.  0.86A   From O4             -0.56 eA-3
PLAT977_ALERT_2_C Check Negative Difference Density on H3C15            -0.40 eA-3
PLAT977_ALERT_2_C Check Negative Difference Density on H1C23A           -0.41 eA-3

Alert level G
FORMU01_ALERT_1_G  There is a discrepancy between the atom counts in the
            _chemical_formula_sum and _chemical_formula_moiety. This is
            usually due to the moiety formula being in the wrong format.
            Atom count from _chemical_formula_sum:   C44.836 H83.67399 Ba7 O33.8
            Atom count from _chemical_formula_moiety:
FORMU01_ALERT_2_G  There is a discrepancy between the atom counts in the
            _chemical_formula_sum and the formula from the _atom_site* data.
            Atom count from _chemical_formula_sum:C44.836 H83.67399 Ba7 O33.892
            Atom count from the _atom_site data:  C44.83800 H79.89199 Ba7 O33.89
CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected.
CELLZ01_ALERT_1_G WARNING: H atoms missing from atom site list. Is this intentional?
           From the CIF: _cell_formula_units_Z    4
           From the CIF: _chemical_formula_sum  C44.836 H83.674 Ba7 O33.892
           TEST: Compare cell contents of formula and atom_site data

           atom    Z*formula  cif sites diff
           C        179.34    179.35   -0.01
           H        334.70    319.57   15.13
           Ba        28.00     28.00    0.00
           O        135.57    135.57    0.00
PLAT004_ALERT_5_G Polymeric Structure Found with Maximum Dimension          3 Info
PLAT005_ALERT_5_G No Embedded Refinement Details Found  in the CIF     Please Do !
PLAT042_ALERT_1_G Calc. and Reported MoietyFormula Strings  Differ     Please Check
PLAT066_ALERT_1_G Predicted and Reported Tmin&Tmax Range Identical          ? Check
PLAT143_ALERT_4_G s.u. on c - Axis Small or Missing ..............    0.00030 Ang.
PLAT301_ALERT_3_G Main Residue  Disorder ..............(Resd  1  )         4% Note
PLAT302_ALERT_4_G Anion/Solvent/Minor-Residue Disorder (Resd  2  )       100% Note
PLAT302_ALERT_4_G Anion/Solvent/Minor-Residue Disorder (Resd  3  )       100% Note
PLAT432_ALERT_2_G Short Inter X...Y Contact  C15      ..C24A             2.48 Ang.
                                                x,1-y,1/2+z  =      7_565 Check
PLAT432_ALERT_2_G Short Inter X...Y Contact  C24B     ..C24B             2.79 Ang.
                                                1-x,y,1/2-z  =      3_655 Check
PLAT720_ALERT_4_G Number of Unusual/Non-Standard Labels ..........         43 Note
PLAT780_ALERT_1_G Coordinates do not Form a Properly Connected Set     Please Do !
PLAT860_ALERT_3_G Number of Least-Squares Restraints .............          7 Note
PLAT910_ALERT_3_G Missing # of FCF Reflection(s) Below Theta(Min).          4 Note
PLAT912_ALERT_4_G Missing # of FCF Reflections Above STh/L=  0.600        482 Note
PLAT960_ALERT_3_G Number of Intensities with I  <   - 2*sig(I) ...          2 Check
PLAT978_ALERT_2_G Number C-C Bonds with Positive Residual Density.          2 Info

   1 ALERT level A = Most likely a serious problem - resolve or explain
   2 ALERT level B = A potentially serious problem, consider carefully
  18 ALERT level C = Check. Ensure it is not caused by an omission or oversight
  21 ALERT level G = General information/check it is not something unexpected

  10 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
  18 ALERT type 2 Indicator that the structure model may be wrong or deficient
   7 ALERT type 3 Indicator that the structure quality may be low
   5 ALERT type 4 Improvement, methodology, query or suggestion
   2 ALERT type 5 Informative message, check

---

Computing details

Data collection: CrysAlis PRO (Rigaku OD, 2019); cell refinement: CrysAlis PRO (Rigaku OD, 2019); data reduction: CrysAlis PRO (Rigaku OD, 2019); program(s) used to solve structure: SHELXT (Sheldrick, 2015); program(s) used to refine structure: JANA2006 (Petříček et al., 2014); molecular graphics: DIAMOND (Brandenburg, 2015) and Origin (Origin, 2000); software used to prepare material for publication: JANA2006 (Petříček et al., 2014).

Poly[[tetradecakis(µ-propionato)heptabarium] propionic acid monosolvate tetrahydrate]

Crystal data

[Ba7(C3H5O2)14]·0.946C3H6O2·4H2O	F(000) = 4063.4
Mr = 2126.4	Dx = 2.090 Mg m^−3
Orthorhombic, Pbcn	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2n 2ab	Cell parameters from 70680 reflections
a = 15.7831 (2) Å	θ = 2.8–29.6°
b = 14.0136 (2) Å	µ = 4.10 mm^−1
c = 30.5583 (3) Å	T = 95 K
V = 6758.83 (15) Å^3	Prism, colourless
Z = 4	0.22 × 0.12 × 0.10 mm

Data collection

Rigaku Oxford Diffraction SuperNova, Dual, Cu at home/near, AtlasS2 diffractometer	8981 independent reflections
Radiation source: X-ray tube	8215 reflections with I > 3σ(I)
Mirror monochromator	Rint = 0.043
Detector resolution: 5.2027 pixels mm^-1	θmax = 29.6°, θmin = 2.4°
ω scans	h = −19→21
Absorption correction: multi-scan (CrysAlisPro; Rigaku OD, 2019)	k = −18→18
Tmin = 0.568, Tmax = 0.656	l = −40→41
112254 measured reflections

Refinement

Refinement on F^2	196 constraints
R[F > 3σ(F)] = 0.028for R[I>3σ (I)]	H atoms treated by a mixture of independent and constrained refinement
wR(F) = 0.071	Weighting scheme based on measured s.u.'s w = 1/(σ^2(I) + 0.0004I^2)
S = 1.92	(Δ/σ)max < 0.001
8981 reflections	Δρmax = 1.14 e Å^−3
428 parameters	Δρmin = −0.72 e Å^−3
7 restraints

Special details

Refinement. 1) Reliability factors considering full occupation of the disordered propionic acid molecule: _refine_ls_R_factor_gt (0.0277), _refine_ls_wR_factor_gt (0.0698), _refine_ls_R_factor_all (0.0324), _refine_ls_wR_factor_ref (0.0712), _refine_ls_goodness_of_fit_ref (1.93), _refine_ls_goodness_of_fit_gt (1.98).

2) Details of the disorder in the proprionic acid molecule: The overall occupational parameter of the disordered propionic acid molecule was determined by refinement of the molecular part comprising of the atoms O15, O16 and C23 which seemed to be the ones least-affected by disorder or overlapping. This refined value has then been used as a value to which the sum of partial occupational parameters of the methyl atoms C24a and C24b should equal while refining the occupational parameter of C24b. The displacement parameter of C24b due to its proximity was supposed to be equal to that of C22 which was refined.

The positions of the methylene hydrogen atoms of C23a and C23b H1C23a, H2C23a; H1C23b, H2C23b) were calculated, with occupational parameters constrained to be equal to the occupational parameters of C24a and C24b, respectively, and with C—H = 0.99Å, U_iso(H) = 1.2U_eq(C). The distance C22—C23 was restrained to 1.52 (1) Å while the distances C23—C24a and C23—C24b were restrained to 1.50 (1) Å.

3) 43 diffractions with (Iobs-Icalc)/sigma(w)>10 were discarded from the refinement:

0 8 0; 6 4 1; 7 7 2; 1 8 2; 5 8 2; 6 8 2; 7 8 2; 2 10 2; 7 4 3; 8 1 4; 4 10 4; 3 4 5; 7 4 5; 6 6 6; 1 10 6; 5 10 6; 6 3 7; 3 4 7; 6 8 8; 0 10 8; 6 2 9; 1 3 9; 3 4 9; 6 6 9; 7 10 10; 5 1 11; 7 1 2; 3 3 12; 1 1 13; 5 1 13; 3 4 13; 4 5 13; 1 2 15; 1 6 15; 4 1 16; 0 2 17; 0 6 17; 1 1 19; 1 2 19; 3 4 21; 1 4 22; 1 1 25; 0 2 25.

4) An alternative refinement of the structure with the disordered propionic acid molecule being removed was carried out with SHELXL (Sheldrick, 2015b) using the SQUEEZE option in PLATON (Spek, 2015). The refinement converged with the folowing reliability factors: _refine_ls_R_factor_all = 0.0308, _refine_ls_R_factor_gt = 0.0280, _refine_ls_wR_factor_ref = 0.0584, _refine_ls_wR_factor_gt = 0.0577, 385 parameters, 9024 diffractions, 4 restraints, condition for the observed diffractions I_obs>2σ(I_obs).

These values are slightly better than those obtained from the refinement with JANA2006 (Petříček et al., 2014) with the same conditions for the observed diffractions I_obs>2σ(I_obs): _refine_ls_R_factor_all = 0.0324, _refine_ls_R_factor_gt = 0.0291, _refine_ls_wR_factor_ref = 0.0710, _refine_ls_wR_factor_gt = 0.0703, 428 parameters, 8981 diffractions, 7 restraints, 196 constraints. However, the refinement with JANA2006 did not include 4 × 4 × 0.946 electrons per unit cell into the calculation because the positions of the hydroxy as well as of the methyl hydrogen atoms of propionic acid were not determined.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
Ba1	0.265102 (12)	0.276842 (14)	0.409817 (6)	0.01040 (6)
O1	0.20473 (14)	0.15684 (17)	0.48047 (7)	0.0141 (7)
O2	0.20378 (14)	0.31250 (17)	0.49391 (7)	0.0160 (7)
C1	0.19826 (19)	0.2274 (3)	0.50646 (10)	0.0139 (10)
C2	0.1819 (2)	0.2043 (3)	0.55457 (10)	0.0194 (11)
H1c2	0.125429	0.174223	0.557629	0.0233*
H2c2	0.221038	0.153268	0.564196	0.0233*
C3	0.1884 (3)	0.2883 (3)	0.58557 (11)	0.0265 (12)
H1c3	0.170755	0.268526	0.614948	0.0397*
H2c3	0.247161	0.310864	0.586517	0.0397*
H3c3	0.151542	0.339958	0.575311	0.0397*
O3	0.77274 (14)	0.27521 (18)	0.67975 (7)	0.0165 (7)
O4	0.70280 (16)	0.13907 (18)	0.67159 (8)	0.0216 (8)
C4	0.7343 (2)	0.2046 (3)	0.69537 (10)	0.0161 (10)
C5	0.7235 (3)	0.1981 (3)	0.74443 (11)	0.0272 (13)
H1c5	0.706908	0.132246	0.752502	0.0327*
H2c5	0.675065	0.238198	0.753611	0.0327*
C6	0.8025 (3)	0.2269 (3)	0.77026 (11)	0.0310 (13)
H1c6	0.79028	0.223693	0.801666	0.0465*
H2c6	0.849043	0.183217	0.763236	0.0465*
H3c6	0.818705	0.29217	0.762411	0.0465*
Ba2	0.596864 (11)	0.480169 (14)	0.553971 (6)	0.00925 (6)
O5	0.39730 (13)	0.31291 (17)	0.46155 (7)	0.0149 (7)
O6	0.50137 (14)	0.39354 (17)	0.49305 (7)	0.0170 (7)
C7	0.45768 (19)	0.3181 (2)	0.48840 (9)	0.0124 (9)
C8	0.4801 (2)	0.2324 (3)	0.51561 (11)	0.0221 (11)
H1c8	0.519283	0.251628	0.539298	0.0266*
H2c8	0.511697	0.185977	0.497441	0.0266*
C9	0.4028 (2)	0.1839 (3)	0.53535 (12)	0.0265 (12)
H1c9	0.421114	0.132078	0.554706	0.0397*
H2c9	0.369982	0.230539	0.55218	0.0397*
H3c9	0.367423	0.15771	0.511864	0.0397*
O1w	0.69585 (16)	0.53342 (18)	0.47792 (8)	0.0176 (8)
H1o1w	0.720 (2)	0.4835 (17)	0.4845 (14)	0.0264*
H2o1w	0.730 (2)	0.575 (2)	0.4853 (13)	0.0264*
O2w	0.43714 (16)	0.4553 (2)	0.59034 (8)	0.0263 (9)
H1o2w	0.398 (2)	0.454 (3)	0.5728 (12)	0.0395*
H2o2w	0.419 (3)	0.472 (3)	0.6140 (8)	0.0395*
Ba3	0.723298 (12)	0.460242 (14)	0.675708 (6)	0.01063 (6)
O7	0.32899 (14)	0.09999 (17)	0.39377 (7)	0.0146 (7)
O8	0.26230 (14)	−0.02799 (17)	0.41819 (8)	0.0147 (7)
C10	0.3271 (2)	0.0247 (2)	0.41603 (10)	0.0124 (9)
C11	0.4054 (2)	−0.0038 (3)	0.44141 (13)	0.0280 (13)
H1c11	0.396235	0.00861	0.472953	0.0336*
H2c11	0.413213	−0.07378	0.439522	0.0336*
C12	0.4852 (2)	0.0456 (3)	0.42663 (16)	0.0426 (17)
H1c12	0.501238	0.022104	0.397576	0.0639*
H2c12	0.475349	0.114565	0.425252	0.0639*
H3c12	0.530935	0.03221	0.447435	0.0639*
O9	0.57946 (15)	0.58185 (18)	0.69864 (7)	0.0184 (7)
O10	0.61677 (15)	0.58789 (17)	0.62908 (7)	0.0152 (7)
C13	0.5694 (2)	0.6136 (2)	0.66061 (11)	0.0159 (10)
C14	0.4989 (2)	0.6848 (3)	0.65013 (13)	0.0311 (13)
H1c14	0.502517	0.70361	0.618957	0.0373*
H2c14	0.443144	0.653296	0.653563	0.0373*
C15	0.5020 (3)	0.7718 (4)	0.67817 (18)	0.0504 (19)
H1c15	0.459821	0.817969	0.667909	0.0756*
H2c15	0.489699	0.754313	0.708558	0.0756*
H3c15	0.558621	0.800339	0.676466	0.0756*
O11	0.62289 (13)	0.33741 (17)	0.61727 (7)	0.0127 (7)
O12	0.57444 (14)	0.35474 (18)	0.68509 (7)	0.0177 (7)
C16	0.5717 (2)	0.3152 (2)	0.64849 (10)	0.0147 (10)
C17	0.5076 (3)	0.2391 (3)	0.63987 (13)	0.0366 (14)
H1c17	0.536797	0.177233	0.635543	0.0439*
H2c17	0.479622	0.251292	0.611423	0.0439*
C18	0.4407 (4)	0.2285 (4)	0.67540 (16)	0.069 (2)
H1c18	0.404027	0.174063	0.668575	0.1033*
H2c18	0.468423	0.217922	0.703673	0.1033*
H3c18	0.406464	0.286802	0.676826	0.1033*
Ba4	0.5	0.45639 (2)	0.75	0.01352 (8)
O13	0.68012 (16)	0.44722 (19)	0.76008 (7)	0.0211 (8)
O14	0.61403 (16)	0.4787 (2)	0.82236 (8)	0.0269 (9)
C19	0.6806 (2)	0.4662 (3)	0.80085 (11)	0.0192 (11)
C20	0.7660 (2)	0.4712 (3)	0.82319 (11)	0.0248 (13)
H1c20	0.808934	0.494763	0.802197	0.0298*
H2c20	0.785871	0.405822	0.829933	0.0298*
C21	0.7687 (2)	0.5316 (3)	0.86451 (12)	0.0225 (12)
H1c21	0.82734	0.536988	0.874707	0.0338*
H2c21	0.746258	0.595323	0.858178	0.0338*
H3c21	0.734129	0.501355	0.887271	0.0338*
C22	0.4426 (5)	−0.0002 (7)	0.2770 (3)	0.031 (4)	0.473 (4)
C24a	0.508 (2)	0.062 (4)	0.2061 (7)	0.16 (2)	0.304 (15)
C24b	0.533 (2)	−0.014 (2)	0.2077 (7)	0.031 (4)	0.169 (15)
H1c23a	0.552935	0.078307	0.268738	0.0718*	0.304 (15)
H2c23a	0.562725	−0.025336	0.251889	0.0718*	0.304 (15)
H1c23b	0.524842	0.099005	0.249815	0.0718*	0.169 (15)
H2c23b	0.572777	0.014063	0.270039	0.0718*	0.169 (15)
O15	0.3759 (5)	0.0388 (6)	0.2758 (2)	0.050 (3)	0.473 (4)
O16	0.4501 (8)	−0.0790 (10)	0.2993 (4)	0.071 (3)	0.473 (4)
C23	0.5222 (10)	0.0286 (11)	0.2521 (6)	0.060 (5)	0.473 (4)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ba1	0.01365 (10)	0.00916 (11)	0.00838 (10)	−0.00298 (7)	−0.00251 (6)	0.00078 (7)
O1	0.0172 (11)	0.0147 (13)	0.0103 (11)	−0.0051 (10)	−0.0004 (8)	−0.0024 (9)
O2	0.0184 (12)	0.0152 (13)	0.0143 (12)	−0.0012 (10)	0.0011 (9)	0.0008 (9)
C1	0.0091 (15)	0.0207 (19)	0.0118 (16)	−0.0031 (13)	−0.0017 (11)	−0.0001 (13)
C2	0.0243 (19)	0.020 (2)	0.0139 (17)	0.0002 (15)	−0.0026 (13)	0.0002 (13)
C3	0.043 (2)	0.023 (2)	0.0128 (17)	0.0025 (18)	0.0039 (15)	−0.0018 (14)
O3	0.0211 (13)	0.0181 (14)	0.0104 (12)	0.0062 (10)	0.0022 (9)	0.0031 (9)
O4	0.0291 (14)	0.0141 (14)	0.0216 (13)	0.0038 (11)	0.0049 (10)	0.0003 (10)
C4	0.0210 (18)	0.0154 (19)	0.0118 (16)	0.0085 (14)	0.0039 (12)	0.0006 (13)
C5	0.043 (2)	0.025 (2)	0.0132 (18)	−0.0031 (18)	0.0071 (15)	0.0051 (15)
C6	0.049 (3)	0.030 (2)	0.0146 (18)	0.007 (2)	−0.0027 (16)	0.0009 (16)
Ba2	0.00957 (10)	0.00981 (11)	0.00836 (10)	−0.00025 (7)	−0.00123 (6)	−0.00020 (7)
O5	0.0169 (12)	0.0160 (13)	0.0118 (11)	−0.0008 (10)	−0.0045 (8)	0.0012 (9)
O6	0.0163 (12)	0.0137 (13)	0.0211 (12)	−0.0008 (10)	−0.0078 (9)	−0.0027 (9)
C7	0.0123 (15)	0.0139 (17)	0.0110 (15)	0.0021 (13)	0.0009 (11)	−0.0033 (12)
C8	0.0190 (18)	0.018 (2)	0.030 (2)	0.0020 (15)	−0.0033 (14)	0.0085 (15)
C9	0.0220 (19)	0.024 (2)	0.034 (2)	−0.0054 (16)	−0.0079 (15)	0.0145 (17)
O1w	0.0204 (13)	0.0160 (14)	0.0162 (12)	−0.0027 (11)	−0.0002 (10)	−0.0005 (10)
O2w	0.0137 (13)	0.0527 (19)	0.0125 (13)	−0.0020 (12)	0.0019 (9)	0.0017 (12)
Ba3	0.01169 (10)	0.01076 (11)	0.00942 (10)	−0.00040 (7)	0.00187 (6)	−0.00148 (7)
O7	0.0172 (12)	0.0134 (12)	0.0132 (11)	−0.0022 (10)	−0.0025 (9)	0.0022 (9)
O8	0.0138 (12)	0.0120 (13)	0.0183 (12)	0.0010 (9)	0.0025 (9)	−0.0003 (9)
C10	0.0108 (15)	0.0144 (17)	0.0122 (16)	0.0017 (13)	−0.0001 (11)	−0.0040 (12)
C11	0.025 (2)	0.024 (2)	0.035 (2)	0.0055 (17)	−0.0136 (16)	0.0035 (17)
C12	0.014 (2)	0.039 (3)	0.075 (4)	−0.0002 (19)	−0.018 (2)	0.001 (2)
O9	0.0226 (13)	0.0167 (13)	0.0160 (12)	−0.0012 (11)	0.0052 (9)	0.0005 (10)
O10	0.0197 (12)	0.0160 (13)	0.0100 (11)	−0.0027 (10)	0.0002 (9)	−0.0001 (9)
C13	0.0175 (16)	0.0118 (17)	0.0184 (17)	−0.0030 (14)	0.0017 (13)	−0.0014 (13)
C14	0.024 (2)	0.031 (2)	0.038 (2)	0.0067 (18)	0.0017 (16)	−0.0008 (18)
C15	0.036 (3)	0.041 (3)	0.074 (4)	0.014 (2)	−0.008 (2)	−0.016 (3)
O11	0.0121 (11)	0.0153 (13)	0.0106 (11)	0.0013 (9)	0.0032 (8)	0.0008 (8)
O12	0.0168 (12)	0.0208 (14)	0.0154 (12)	−0.0028 (11)	0.0048 (9)	−0.0055 (9)
C16	0.0157 (16)	0.0146 (18)	0.0137 (16)	−0.0009 (14)	0.0046 (12)	−0.0008 (12)
C17	0.040 (2)	0.039 (3)	0.031 (2)	−0.026 (2)	0.0169 (18)	−0.0183 (19)
C18	0.073 (4)	0.071 (4)	0.062 (3)	−0.061 (4)	0.046 (3)	−0.035 (3)
Ba4	0.01414 (14)	0.01790 (16)	0.00851 (13)	0	0.00393 (9)	0
O13	0.0259 (14)	0.0265 (15)	0.0110 (12)	0.0051 (11)	−0.0003 (10)	−0.0023 (10)
O14	0.0211 (13)	0.048 (2)	0.0111 (13)	0.0057 (13)	0.0015 (10)	0.0005 (11)
C19	0.0256 (19)	0.0198 (19)	0.0123 (17)	0.0049 (15)	0.0013 (13)	0.0010 (13)
C20	0.023 (2)	0.037 (3)	0.0148 (19)	0.0069 (17)	−0.0013 (13)	−0.0007 (16)
C21	0.0209 (19)	0.025 (2)	0.0214 (19)	−0.0045 (16)	−0.0028 (14)	−0.0011 (15)
C22	0.037 (7)	0.028 (5)	0.029 (6)	−0.003 (5)	−0.014 (4)	0.006 (4)
C24a	0.12 (3)	0.23 (5)	0.14 (3)	0.01 (3)	0.05 (2)	0.09 (3)
C24b	0.037 (7)	0.028 (5)	0.029 (6)	0.003 (5)	−0.014 (4)	−0.006 (4)
O15	0.038 (4)	0.057 (5)	0.054 (5)	−0.020 (4)	0.014 (3)	−0.015 (4)
O16	0.037 (4)	0.059 (6)	0.116 (7)	0.000 (4)	0.002 (4)	0.046 (5)
C23	0.050 (11)	0.056 (8)	0.074 (9)	−0.014 (6)	−0.031 (9)	0.027 (7)

Geometric parameters (Å, º)

O1—C1	1.273 (4)	C18—H1c18	0.98
O2—C1	1.256 (4)	C18—H2c18	0.98
C1—C2	1.528 (4)	C18—H3c18	0.98
C2—H1c2	0.99	O13—C19	1.274 (4)
C2—H2c2	0.99	O14—C19	1.251 (4)
C2—C3	1.515 (5)	C19—C20	1.513 (5)
C3—H1c3	0.98	C20—H1c20	0.99
C3—H2c3	0.98	C20—H2c20	0.99
C3—H3c3	0.98	C20—C21	1.521 (5)
O3—C4	1.255 (4)	C21—H1c21	0.98
O4—C4	1.272 (4)	C21—H2c21	0.98
C4—C5	1.512 (5)	C21—H3c21	0.98
C5—H1c5	0.99	C22—O15	1.187 (12)
C5—H2c5	0.99	C22—O16	1.303 (18)
C5—C6	1.529 (6)	C22—C23	1.523 (18)
C6—H1c6	0.98	C24a—C23	1.50 (3)
C6—H2c6	0.98	C24b—C23	1.49 (3)
C6—H3c6	0.98	H1c23a—C23	0.99
O5—C7	1.260 (4)	H2c23a—C23	0.99
O6—C7	1.270 (4)	H1c23b—C23	0.99
C7—C8	1.504 (5)	H2c23b—C23	0.99
C8—H1c8	0.99	Ba1—O1	2.898 (2)
C8—H2c8	0.99	Ba1—O2	2.791 (2)
C8—C9	1.521 (5)	Ba1—O3^i	2.835 (2)
C9—H1c9	0.98	Ba1—O4^i	2.923 (2)
C9—H2c9	0.98	Ba1—O5	2.666 (2)
C9—H3c9	0.98	Ba1—O7	2.720 (2)
O1w—H1o1w	0.82 (3)	Ba1—O8^ii	2.781 (2)
O1w—H2o1w	0.82 (3)	Ba1—O10^iii	2.913 (2)
O2w—H1o2w	0.82 (3)	Ba1—O11^i	2.879 (2)
O2w—H2o2w	0.81 (3)	Ba2—O1^iv	2.774 (2)
O7—C10	1.256 (4)	Ba2—O5^iii	2.940 (2)
O8—C10	1.263 (4)	Ba2—O6	2.685 (2)
C10—C11	1.513 (5)	Ba2—O6^iii	2.757 (2)
C11—H1c11	0.99	Ba2—O1w	2.898 (2)
C11—H2c11	0.99	Ba2—O2w	2.777 (3)
C11—C12	1.507 (6)	Ba2—O8^iv	2.827 (2)
C12—H1c12	0.98	Ba2—O10	2.765 (2)
C12—H2c12	0.98	Ba2—O11	2.813 (2)
C12—H3c12	0.98	Ba3—O3	2.711 (3)
O9—C13	1.255 (4)	Ba3—O4^v	2.767 (3)
O10—C13	1.272 (4)	Ba3—O7^iv	2.829 (2)
C13—C14	1.528 (5)	Ba3—O8^iv	3.084 (2)
C14—H1c14	0.99	Ba3—O9	2.924 (2)
C14—H2c14	0.99	Ba3—O10	2.838 (2)
C14—C15	1.491 (7)	Ba3—O11	2.943 (2)
C15—H1c15	0.98	Ba3—O12	2.791 (2)
C15—H2c15	0.98	Ba3—O13	2.673 (2)
C15—H3c15	0.98	Ba3—O15^iv	2.828 (7)
H1c15—H2c15	1.6003	Ba4—O9	2.670 (2)
H1c15—H3c15	1.6003	Ba4—O9^vi	2.670 (2)
H2c15—H3c15	1.6003	Ba4—O12	2.710 (2)
O11—C16	1.288 (4)	Ba4—O12^vi	2.710 (2)
O12—C16	1.249 (4)	Ba4—O13	2.862 (3)
C16—C17	1.494 (5)	Ba4—O13^vi	2.862 (3)
C17—H1c17	0.99	Ba4—O14	2.868 (2)
C17—H2c17	0.99	Ba4—O14^vi	2.868 (2)
C17—C18	1.522 (7)
O1—C1—O2	122.8 (3)	O2—Ba1—O8^ii	71.65 (7)
O1—C1—C2	116.7 (3)	O2—Ba1—O10^iii	118.77 (6)
O2—C1—C2	120.5 (3)	O2—Ba1—O11^i	95.39 (6)
C1—C2—H1c2	109.47	O3^i—Ba1—O4^i	45.29 (7)
C1—C2—H2c2	109.47	O3^i—Ba1—O5	126.01 (6)
C1—C2—C3	115.2 (3)	O3^i—Ba1—O7	64.90 (7)
H1c2—C2—H2c2	103.07	O3^i—Ba1—O8^ii	110.40 (7)
H1c2—C2—C3	109.47	O3^i—Ba1—O10^iii	75.30 (6)
H2c2—C2—C3	109.47	O3^i—Ba1—O11^i	67.20 (6)
C2—C3—H1c3	109.47	O4^i—Ba1—O5	133.75 (7)
C2—C3—H2c3	109.47	O4^i—Ba1—O7	109.79 (7)
C2—C3—H3c3	109.47	O4^i—Ba1—O8^ii	68.25 (7)
H1c3—C3—H2c3	109.47	O4^i—Ba1—O10^iii	66.77 (7)
H1c3—C3—H3c3	109.47	O4^i—Ba1—O11^i	73.57 (7)
H2c3—C3—H3c3	109.47	O5—Ba1—O7	89.40 (7)
O3—C4—O4	122.7 (3)	O5—Ba1—O8^ii	83.15 (7)
O3—C4—C5	118.6 (3)	O5—Ba1—O10^iii	67.52 (6)
O4—C4—C5	118.6 (3)	O5—Ba1—O11^i	152.39 (7)
C4—C5—H1c5	109.47	O7—Ba1—O8^ii	166.01 (7)
C4—C5—H2c5	109.47	O7—Ba1—O10^iii	106.39 (7)
C4—C5—C6	113.8 (3)	O7—Ba1—O11^i	74.36 (6)
H1c5—C5—H2c5	104.72	O8^ii—Ba1—O10^iii	59.80 (7)
H1c5—C5—C6	109.47	O8^ii—Ba1—O11^i	116.89 (6)
H2c5—C5—C6	109.47	O10^iii—Ba1—O11^i	138.06 (6)
C5—C6—H1c6	109.47	O1^iv—Ba2—O5^iii	127.04 (6)
C5—C6—H2c6	109.47	O1^iv—Ba2—O6	76.61 (7)
C5—C6—H3c6	109.47	O1^iv—Ba2—O6^iii	126.29 (6)
H1c6—C6—H2c6	109.47	O1^iv—Ba2—O1w	62.81 (7)
H1c6—C6—H3c6	109.47	O1^iv—Ba2—O2w	128.49 (8)
H2c6—C6—H3c6	109.47	O1^iv—Ba2—O8^iv	73.22 (7)
O5—C7—O6	122.2 (3)	O1^iv—Ba2—O10	128.55 (7)
O5—C7—C8	119.4 (3)	O1^iv—Ba2—O11	71.28 (6)
O6—C7—C8	118.4 (3)	O5^iii—Ba2—O6	110.59 (7)
C7—C8—H1c8	109.47	O5^iii—Ba2—O6^iii	45.60 (6)
C7—C8—H2c8	109.47	O5^iii—Ba2—O1w	66.41 (7)
C7—C8—C9	112.8 (3)	O5^iii—Ba2—O2w	102.51 (8)
H1c8—C8—H2c8	105.89	O5^iii—Ba2—O8^iv	77.63 (6)
H1c8—C8—C9	109.47	O5^iii—Ba2—O10	65.91 (6)
H2c8—C8—C9	109.47	O5^iii—Ba2—O11	143.89 (6)
C8—C9—H1c9	109.47	O6—Ba2—O6^iii	67.25 (7)
C8—C9—H2c9	109.47	O6—Ba2—O1w	82.13 (7)
C8—C9—H3c9	109.47	O6—Ba2—O2w	73.22 (7)
H1c9—C9—H2c9	109.47	O6—Ba2—O8^iv	146.54 (7)
H1c9—C9—H3c9	109.47	O6—Ba2—O10	152.38 (7)
H2c9—C9—H3c9	109.47	O6—Ba2—O11	103.72 (7)
H1o1w—O1w—H2o1w	104 (3)	O6^iii—Ba2—O1w	73.74 (7)
H1o2w—O2w—H2o2w	109 (4)	O6^iii—Ba2—O2w	77.20 (7)
O7—C10—O8	122.6 (3)	O6^iii—Ba2—O8^iv	121.61 (7)
O7—C10—C11	118.7 (3)	O6^iii—Ba2—O10	98.40 (7)
O8—C10—C11	118.7 (3)	O6^iii—Ba2—O11	153.77 (6)
C10—C11—H1c11	109.47	O1w—Ba2—O2w	147.42 (7)
C10—C11—H2c11	109.47	O1w—Ba2—O8^iv	71.48 (7)
C10—C11—C12	114.1 (3)	O1w—Ba2—O10	117.64 (7)
H1c11—C11—H2c11	104.42	O1w—Ba2—O11	130.99 (7)
H1c11—C11—C12	109.47	O2w—Ba2—O8^iv	138.40 (7)
H2c11—C11—C12	109.47	O2w—Ba2—O10	80.75 (7)
C11—C12—H1c12	109.47	O2w—Ba2—O11	76.60 (7)
C11—C12—H2c12	109.47	O8^iv—Ba2—O10	61.04 (7)
C11—C12—H3c12	109.47	O8^iv—Ba2—O11	80.03 (6)
H1c12—C12—H2c12	109.47	O10—Ba2—O11	78.51 (6)
H1c12—C12—H3c12	109.47	O3—Ba3—O4^v	138.34 (7)
H2c12—C12—H3c12	109.47	O3—Ba3—O7^iv	65.10 (7)
O9—C13—O10	121.8 (3)	O3—Ba3—O8^iv	106.22 (6)
O9—C13—C14	121.2 (3)	O3—Ba3—O9	140.37 (7)
O10—C13—C14	117.0 (3)	O3—Ba3—O10	142.77 (7)
C13—C14—H1c14	109.47	O3—Ba3—O11	67.87 (6)
C13—C14—H2c14	109.47	O3—Ba3—O12	74.39 (7)
C13—C14—C15	112.9 (3)	O3—Ba3—O13	87.95 (7)
H1c14—C14—H2c14	105.79	O3—Ba3—O15^iv	74.66 (16)
H1c14—C14—C15	109.47	O4^v—Ba3—O7^iv	89.29 (7)
H2c14—C14—C15	109.47	O4^v—Ba3—O8^iv	66.10 (6)
C14—C15—H1c15	109.47	O4^v—Ba3—O9	79.07 (7)
C14—C15—H2c15	109.47	O4^v—Ba3—O10	69.89 (7)
C14—C15—H3c15	109.47	O4^v—Ba3—O11	136.80 (6)
H1c15—C15—H2c15	109.47	O4^v—Ba3—O12	147.07 (7)
H1c15—C15—H3c15	109.47	O4^v—Ba3—O13	102.31 (7)
H2c15—C15—H3c15	109.47	O4^v—Ba3—O15^iv	70.16 (16)
O11—C16—O12	122.3 (3)	O7^iv—Ba3—O8^iv	43.61 (6)
O11—C16—C17	117.8 (3)	O7^iv—Ba3—O9	144.26 (6)
O12—C16—C17	119.9 (3)	O7^iv—Ba3—O10	99.24 (6)
C16—C17—H1c17	109.47	O7^iv—Ba3—O11	71.80 (6)
C16—C17—H2c17	109.47	O7^iv—Ba3—O12	114.55 (7)
C16—C17—C18	114.4 (4)	O7^iv—Ba3—O13	148.63 (7)
H1c17—C17—H2c17	104.01	O7^iv—Ba3—O15^iv	83.84 (15)
H1c17—C17—C18	109.47	O8^iv—Ba3—O9	101.45 (6)
H2c17—C17—C18	109.47	O8^iv—Ba3—O10	57.13 (6)
C17—C18—H1c18	109.47	O8^iv—Ba3—O11	73.92 (6)
C17—C18—H2c18	109.47	O8^iv—Ba3—O12	115.25 (6)
C17—C18—H3c18	109.47	O8^iv—Ba3—O13	165.74 (7)
H1c18—C18—H2c18	109.47	O8^iv—Ba3—O15^iv	108.43 (15)
H1c18—C18—H3c18	109.47	O9—Ba3—O10	45.02 (6)
H2c18—C18—H3c18	109.47	O9—Ba3—O11	93.91 (6)
O13—C19—O14	122.6 (3)	O9—Ba3—O12	68.32 (7)
O13—C19—C20	117.1 (3)	O9—Ba3—O13	67.09 (7)
O14—C19—C20	120.3 (3)	O9—Ba3—O15^iv	122.20 (16)
C19—C20—H1c20	109.47	O10—Ba3—O11	75.23 (6)
C19—C20—H2c20	109.47	O10—Ba3—O12	83.50 (7)
C19—C20—C21	115.2 (3)	O10—Ba3—O13	112.10 (7)
H1c20—C20—H2c20	103.1	O10—Ba3—O15^iv	139.87 (16)
H1c20—C20—C21	109.47	O11—Ba3—O12	45.51 (6)
H2c20—C20—C21	109.47	O11—Ba3—O13	114.08 (7)
C20—C21—H1c21	109.47	O11—Ba3—O15^iv	141.20 (16)
C20—C21—H2c21	109.47	O12—Ba3—O13	69.52 (7)
C20—C21—H3c21	109.47	O12—Ba3—O15^iv	131.73 (16)
H1c21—C21—H2c21	109.47	O13—Ba3—O15^iv	73.25 (16)
H1c21—C21—H3c21	109.47	O9—Ba4—O9^vi	97.61 (7)
H2c21—C21—H3c21	109.47	O9—Ba4—O12	73.28 (7)
O15—C22—O16	119.1 (10)	O9—Ba4—O12^vi	168.56 (7)
O15—C22—C23	126.5 (11)	O9—Ba4—O13	68.05 (7)
O16—C22—C23	114.3 (10)	O9—Ba4—O13^vi	115.65 (7)
C22—C23—C24a	115.3 (17)	O9—Ba4—O14	94.96 (7)
C22—C23—C24b	116.0 (17)	O9—Ba4—O14^vi	76.68 (7)
C22—C23—H1c23a	109.47	O9^vi—Ba4—O12	168.56 (7)
C22—C23—H2c23a	109.47	O9^vi—Ba4—O12^vi	73.28 (7)
C22—C23—H1c23b	109.47	O9^vi—Ba4—O13	115.65 (7)
C22—C23—H2c23b	109.47	O9^vi—Ba4—O13^vi	68.05 (7)
C24a—C23—H1c23a	109.47	O9^vi—Ba4—O14	76.68 (7)
C24a—C23—H2c23a	109.47	O9^vi—Ba4—O14^vi	94.96 (7)
C24b—C23—H1c23b	109.47	O12—Ba4—O12^vi	116.58 (7)
C24b—C23—H2c23b	109.47	O12—Ba4—O13	67.95 (7)
H1c23a—C23—H2c23a	102.92	O12—Ba4—O13^vi	109.16 (7)
H1c23b—C23—H2c23b	102.1	O12—Ba4—O14	110.46 (7)
O1—Ba1—O2	45.88 (7)	O12—Ba4—O14^vi	76.42 (7)
O1—Ba1—O3^i	125.73 (7)	O12^vi—Ba4—O13	109.16 (7)
O1—Ba1—O4^i	139.24 (7)	O12^vi—Ba4—O13^vi	67.95 (7)
O1—Ba1—O5	85.73 (6)	O12^vi—Ba4—O14	76.42 (7)
O1—Ba1—O7	74.18 (6)	O12^vi—Ba4—O14^vi	110.46 (7)
O1—Ba1—O8^ii	116.81 (7)	O13—Ba4—O13^vi	174.86 (7)
O1—Ba1—O10^iii	153.16 (6)	O13—Ba4—O14	45.47 (7)
O1—Ba1—O11^i	68.60 (6)	O13—Ba4—O14^vi	135.33 (7)
O2—Ba1—O3^i	161.74 (7)	O13^vi—Ba4—O14	135.33 (7)
O2—Ba1—O4^i	126.49 (7)	O13^vi—Ba4—O14^vi	45.47 (7)
O2—Ba1—O5	72.03 (6)	O14—Ba4—O14^vi	167.46 (9)
O2—Ba1—O7	117.23 (7)

Symmetry codes: (i) x−1/2, −y+1/2, −z+1; (ii) −x+1/2, y+1/2, z; (iii) −x+1, −y+1, −z+1; (iv) x+1/2, −y+1/2, −z+1; (v) −x+3/2, y+1/2, z; (vi) −x+1, y, −z+3/2.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O1w—H1o1w···O1^iv	0.82 (3)	2.25 (3)	2.957 (3)	145 (4)
O1w—H2o1w···O2^iii	0.82 (3)	2.00 (3)	2.813 (3)	171 (3)
O2w—H1o2w···O1w^iii	0.82 (3)	2.15 (3)	2.963 (3)	172 (4)
O2w—H2o2w···O14^vi	0.81 (3)	2.01 (3)	2.807 (3)	164 (4)
C17—H1c17···O16^vii	0.99	2.43	2.989 (15)	115.22

Symmetry codes: (iii) −x+1, −y+1, −z+1; (iv) x+1/2, −y+1/2, −z+1; (vi) −x+1, y, −z+3/2; (vii) −x+1, −y, −z+1.